Treating particulate materials



March 4, 1958 R. F. HEALD TREATING PARTICULATE MATERIALS I 2 Sheets-Sheet 1 Filed Jan. 27-. 1954 'INVENTOR. Rosm'r fRA A/KL //v [/5410 ATTUAIVEY March 4, 1958 R. F. HEALb 2,825,190

' TREATING PARTICULATE! MATERIALS Filed Jan. 27. 1954 2 Sheets-Sheet 2 b k & Y I *1 I? w Q l 2 E A INVENTOR. Roam r RAA/KL /N/-/E/ 1 [0 al/w? W ATTORNEY UniteStates Patent 2,825,190 TREATING PARTICULATE MATERIALS Robert Franklin Heald, Nutley, N. J., assignor to Colgate- Palmolive Company, Jersey City, N. 1., a corporation of Delaware Application January 27, 1954, Serial No- 406,499

7 Claims. (Cl. 53-21) The present invention relates to the introduction of liquids into particulate materials and has more particular reference to a method and apparatus for introducing a predetermined quantity of a mixture of a liquid and a liquefied, normally gaseous, propellant interiorly into a given mass of particulate materials.

Particulate materials or powdered products such as soaps, non-soap synthetic detergents, dental powders, face powders, dusting powders, and the like generally have an aromatic liquid oil or perfume added thereto to increase the appeal of the same to'the public.

Generally, liquid oils or perfumes are incorporated in such products either by adding the same to the powder ina mixing device or in a micropulverizer or the like or by spraying the oil, under air pressure, onto the particles as the latter are being conveyed to storage bins or to packaging stations.

Neither of these perfuming methods has proved to be completely satisfactory because in each instance a relative ly large amount of the perfume is lost to the surrounding atmosphere.

The air spraying or atomization technique described has the further disadvantage in that the perfume, when discharge from the nozzle of the atomizer under the pres sures which are necessary to break the perfume oils into droplets, stirs up powder dust which, in time, builds up on the nozzle obstructing the exit of the orifice therein and preventing satisfactory atomization of the perfume therethrough.

The present invention provides a method and apparatus for distributing liquids such as perfumes in powders which overcomes or substantially minimizes the disadvantages of the prior art methods described hereinabove.

In the broadest process aspects thereof the present invention provides a method which comprises introducing a predetermined quantity of a mixture of a liquid and a liquefied, normally gaseous propellant interiorly into a given mass of particulate material.

Broadly, the apparatus of this invention comprises a container adapted to maintain a mixture of a liquid and a liquefied, normally gaseous propellant in liquid form, a nozzle in communication with said container adapted for 'reciprocable movement in and out of a mass of particulate material, means for reciprocating the nozzle, and means for permitting a predetermined quantity of said liquid mixture to pass from said container and out through said nozzle only when the nozzle is in said mass of particulate material.

While the invention is applicable broadly to the distribution of liquids, e. g., oils, fats, and the like of various types in particulate products of many kinds, it will be described with particular reference to the perfuming of detergent compositions in particulate form, i. e., powders, beads, or the like.

Particulate detergent products generally are packaged commercially in cartons on automatic filling machines. Such machines differ considerably in structural detail but all such commercial machines have a number of stations to which the cartons are moved in sequence. Special reference will be had, in the following description of the method and apparatus of therinvention, to the way of performing the steps in a machine including a detergent filling station and a perfuming station.

The advantages of the process and apparatus will become apparent from the following detailed description of the invention taken in conjunction with the accompanying drawings in which:

Fig. 1 depicts in diagrammatic form a view, partly in perspective and partly broken away for greater clarity, of apparatus embodying features of the invention;

Fig. 2 is a viewshowing in schematic form a wiring diagram for parts of the apparatus associated with controlling the reciprocable movement of a discharge nozzle in accordance with this invention; and

Fig. 3 is an enlarged sectional view showing the outlet end of a reciprocating discharge nozzle and a valve assembly for controlling the flow through such nozzle of a mixture of a liquid and a liquefied, normally gaseous propellant in accordance with this invention.

Referring now more particularly to Fig. 1, reference numeral 10 refers to a detergent or powder hopper which may be secured to a bracket or a standard (not shown) of any convenient design. The hopper has a discharge nozzle 14 at its lower end. If desired, an auger may be mounted for rotation within said nozzle to aid in discharging powder therethrough. Below the powder discharge nozzle 14 is a conveyor beltor chain 16 having carton cups 18 mounted thereon. Conveyor 16 is adapted to move intermittently a distance corresponding to the distance between cups 18 and successively position empty detergent cartons 20 beneath the discharge nozzle 14.

The parts thus far described are elements of a conventional and well known type of detergent carton filling machine, whose structure and operation are well known to those familiar with this art. Briefly stated, the filling machine is provided with a drive mechanism (not shown) for moving the belt as-described to convey an empty detergent carton 20 into a position of rest beneath nozzle 14 as shown on the drawing. During the dwell in the movement of the conveyor belt 16, the valves (not shown) controlling the feed of the detergent material with which the cartons are to be filled are opened automatically.

The filling machine operates on a volumetric basis to introduce a predetermined quantity of detergent particles into the carton. When the predetermined quantity of particles has been filled into the carton, the valve mechanism automatically shuts ofi and the conveyor then moves in the direction of the arrows to position the next empty carton beneath the filling nozzle 14. The filled detergent carton 22 also is moved along a corresponding distance to the right by the conveyor belt 16, as shown on the draw- The perfuming device of this invention comprises a bracket 28 secured to a supporting standard (not shown) of any convenient design. The bracket 28 hasa laterally projecting guide arm 30 provided'with a centrally apertured head 32 on its free end. Arm 30 is of such a length that head 32 on the free end thereof is located substantially directly above the position which is occupied by a'filled detergent carton while the next succeeding carton 20 is being filled, i. e., the next position of rest into which a filled detergent carton moves after it leaves the filling station.

;An air cylinder 34 is secured to bracket 28 in any suitable manner, e. g., as by welding, bolting, or the like. A shaft 36 extends longitudinally through cylinder 34 and carries a piston 38. The shaft and piston are adapted for reciprocal motion within the cylinder. The 'shaft passes through a stufiing box located at the top of the cylinder 34.

An elevator 46 is secured'to the upper end of shaft 36 and has a laterally extending arm 48 having an aperture '50 near its free end and an actuating member 51 (the function of which will 'be described below) on its free end. Arm '48 is of such a length that the aperture ispositioned directly above and in vertical alignment withthe aperture in head 32 on arm 30 when'the respective parts are in operative assemblage.

Avertically-extending guide rod 52, threaded at its upper end intoa'rm '48 on elevator 46, is relatively movable within guide holes 56 and 58 on bracket 28 as shown on the drawing.

The'ends 60 and 62 of a pai'rof airlines, '64 and 66, enter'air'cylinder 34 at the top and 'bottom thereof, respectively. The 'other'ends'68'and of lines 64 and '66- are located in a block 71. Air under pressure of'about '5090 *poundsperisquare inch is delivered to air lines '64 and from an air compressor 74 through a control valve 76. Valve 76 comprises a'solid block 78 having an air inlet passage 80 which divides within the block 78 into two outlet passages 82 and 84. Block 78 is connectedto a solenoid 86 through a link 88 and is adapted for lateral reciprocal motion beneath block 71 on a guide 90 mounted on a frame (not'shown).

One end of a flexiblehose 92 is connected with inlet passage 80 and the otherend is connected to the air compressor 74 through a line 94. The exit 'ends of passages '82 and 84 are located in block 78, with respect to the-ends 70 and 68 of air lines 66 and 64 in block 71, in-suc'h manner that when theexit end of one of the'passages, e. g., 84, and the end of one of the air lines, e. g., end '68 of line 64 are in registry, the end of the other air line, :2. g., end 70 of line 66, is open to the atmosphere and the exit end of the other passage, e. g., 82, is closed by -block'71, as 'shown on the drawing.

A thin elongated tube or nozzle 96 having a restrictive passageway 185 is located within apertures in heads 32'and 50. 'The nozzle has a sliding fit in the aperture in head 32. A set screw 98 -or like means is provided for:'securing-the nozzle 96 in aperture 50 at any desired position.

A stop 100, shown moreclearlyin Fig. 2, is mounted on nozzle 96 and maintainedat any desired location along said nozzle by set screw 104or by like means. Stop is adapted, through vertical reciprocable movement of nozzle 96, tocontact brackets 108 and 110. Each of the brackets 108--and 110 is adapted for vertical reciprocable movement on a fixed rod 112 secured to a suitable supporting standard (not shown). Brackets 108 and 110 are connected by a pair of links 114 and 116. A pin 118 serves to secure one of the ends of each link to bracket 108. Bracket 110 has a pair of fingers 120 and 122 extending outwardly therefrom which are adapted to receive a pin 124. Pin 124 is adapted to move freely within the longitudinal slot defined by fingers 120 and 122 and has the other ends of links 114 and 116 secured thereto as illustrated on the drawing.

A pair of switches 126 and -1'28 are mounted on a support (not shown) of any suitable design. Switch 126 has an actuating member 130 maintained in its outermost or closed position by the outward force exerted thereon by a coiled spring 132. Member 130 is secured rremovably to bracket 110 by a pin 134. Switch 126 is of such a design that it is open only when member 130 thereof has been moved interiorly of the switch into the position shown in dottedlines on the drawing. 0 Switch 128 has an actuating member 138 maintained 1n 1ts innermost or closed position by the upward force exerted thereon by bracket .108. Member 138 is secured irremovably to bracket108 by a'pin 140, Switch 128 i ofsuch a design that it is openonly when-member 138 thereof has been'moved outwardly of swirtoh'1-28.

The discharge end of nozzle 96, shown rnore clearly in Fig. 3, is provided with an outlet or orifice 144 which is about 0.02 to about 0.10 centimeter in diameter. The nozzle 96, restricted passageway 185 and outlet 144 are all substantially less in cross-sectional area than the mass of particulate material. This facilitates entry of the nozzle and restricted passageway into the mass of particulate material without compacting, compressing or breaking up the particles. It also slows the discharge of perfume solution and thereby allows better control of the dispensing of the relatively small quantities employed. ,A restricted passageway and outlet also promote spray dispensing rather than stream dispensing, due to the turbulent flow obtainedin the former case. It is preferred to taper the lower end of nozzle 96, as illustrated at 146, to facilitate entry of the same into the filled detergent carton 22. Outlet orifice 144 may be located at any convenient position in the lower portion of nozzle 96 although it is preferred that it be located in the side wall of the nozzle near the tapered end 146 as illustrated on the drawing. Orifice 144 should'not be located on the tip of nozzle 96 since if so located it might become clogged with detergent particles when the nozzle is inserted into a filled carton.

Looking again at Fig. 1, to the other end of nozzle 96 is attached one end of a flexible tube 148. The other end of tube 148 is fastened to one end of a pipe 150 whose other end is connected by coupling 152, to a perfume charge cylinder 154 secured to a bracket 156. Cylinder 154 is provided with a valve 158 which may be formed integral therewith. Coupling 152 permits -removal of cylinder 154 from pipe 150 when it is necessary to recharge the cylinder. The liquid mixture is introduced into the cylinder, during charging thereof, through valve 158. After cylinder 154 has been connected to pipe 150 through coupling 152 valve 158 is opened to permit .the'material to enter pipe 150.

A'needle valve 160, shown'more clearly in Fig. 3, is located in nozzle 96 near the outlet 'orific'e 144 therein. Theneedle 162 of valve is connected with a threaded rod 164 adapted 'for reciprocable movement in a solenoid 166. A coiled spring 167 exerts an outward force on rod and serves .to urge the needle 162 of valve 160 tightly against its seat 168.

Turning again to Fig. 1, a switch 169 having a resilient trigger 170 is connected in series with solenoid 166. A spring 172 normally maintains trigger 170 in its open position shown in dotted lines on the drawing. Switch 169 is mounted on a suitable support (not shown) in such manner that the actuating member 51 on arm 48 will contact and 'move'the same into the position shown in solid lines on the drawing as the nozzle is moved in and out of the cartons thus opening and closing valve 160.

Looking now at Fig. 3, a lock nut 174 or like adjustable means, thre'aded-on rod 164, serves to limit the distance through which rod 164 may travel. Since needle 162 of valve 160 'is connected with rod 164 it is possible, by changing the/position of nut 174 on the rod, to regulate the size of the opening in valve 160 and thereby control the amount of'rnaterial which will pass from cylinder 154 into tube 148 and out of the orifice 144 of nozzle 96.

As shown in Figs. 1 and 2, a lamp 176, located on one side of conveyor 16, projects a beam of light 177 across the conveyor at a height such that it will be interrupted by cartons passing along on the conveyor. Light sensitive means such as a photoelectric cell 178 is positioned on the other sideof the conveyor in such manner as to receive'the beam when the latter is not interrupted.

The coil of a relay 180 derives its power from the photoelectric cell 178 through an amplifier 179. The contacts of relay 180 and switches 126 and .128 are connected in series with solenoid 86 as shown on the drawing, Solenoid86 hasaplunger 182 and a coiled spring 184. One end of link 88 is connected with the freeend As long asiight beam 177 remains uninterrupted the relay 180 remains open and the circuit including solenoid 86 and switches 126 and 128 necessarily remains open. When this circuit is open, no current flows through solenoid 86 and the same is de-energized. Under these conditions the outward force exerted on plunger 182 by spring 184 maintains the plunger in its outermost position with reference to solenoid 86. When the plunger is in its outermost position block 78 is maintained, by link 88, in a position such that the outlet end of passage 82 in block 78 and the end 70 of line 66 are in registry, the' end 68 of line 64 is open to the atmosphere, andthe outlet end of passage 84 is closed by block 71.

-When the parts are in the respective positions just described air under pressure from compressor 74 enters the cylinder below piston 38 and forces the piston upwardly. When piston 38 is in its uppermost position nozzle 96 also is in its uppermost position through the interconnection of these parts with shaft 36 and elevator 46. When nozzle 96 is in its uppermost position as just described, stop 100 maintains bracket 108 in its uppermost position whereby switch 128' is closed. Also, spring 132 urges member 130 outwardly of switch 126 whereby that switch is closed. The various parts will remain in the respective positions described until the electrical circuit is closed, e. g., by the'interruption of beam 177 by a carton.

The practicing of the present process using the apparatus of this invention now will be described-with respect to the packaging in cartons andp'erfuming therein of acids contained in coconut oil.

In accordance with this invention spray dried soap beads of the character described are introduced into hopper 10, a mixture containing about 25% perfume and about 75% propellant, the latter comprising about 60% dichlorotetrofluorethane and about 40% dichlorodifluoromethane, is introduced into cylinder 154, and empty cartons 20 are placed in cups 18 on conveyor 16 with their open ends up.

The drive mechanism which is adapted to. move the conveyor intermittently then is started whereupon an empty carton 20 is moved into a position of rest beneath nozzle 14 of hopper 10. During the dwell in the movement of the conveyor, the valves controlling the passage of soap beads through nozzle 14 are opened automatically and a predetermined quantity of beads are filled into the carton. The valve mechanism then shuts ofi automatically and the conveyor drive mechanism then automatically moves'the conveyor 16 in the direction of the arrows as indicated'on the drawing. The conveyor spray dried soap beads prepared from the higher fatty mechanism then shuts off and the conveyor again comes to rest with the next empty carton positioned beneath nozzle 14. The movement of theconveyor to position said next empty carton beneath nozzle 14 also moves the filled carton 22' into a position of rest beneath nozzle 96. It will be apparent that as carton 22 moves into pressor 74, through line 94, hose 92, passages'80 and 84, air line 64 and into the space in cylinder 34 above piston 38 and force the piston downwardly. The downward movement of piston 38 forces air in the space below the piston out the cylinder through the end 70 of line 66 and then to the atmosphere.

As piston 38 moves downwardly, the shaft 36 and elevator 46 also move downwardly. Since nozzle 96 is connected fixedly in aperture 50 in arm 48 byset screw 98, the downward movement of the piston 38 and shaft 36 is paralleled by the downward movement of nozzle 96 which enters the open end of the filled carton 22.

-As nozzle 96 moves downwardly into the carton, mem-. ber 51 on arm 48 of the elevator 46 contacts resilient trigger 170 causing the same to move into the position shown in solid lines on the drawing and close switch 169 and the circuit including solenoid 166. With the closing of this circuit solenoid 166 is energized moving rod 164 inwardly of the solenoid thereby moving needle 162 away from seat 168 opening valve 160. With the opening of valve 160 the material in cylinder 154 passes into the soap beads through orifice 144 in nozzle 96, being discharged from the outlet as a spray.

As nozzle 96 continues to move downwardly stop 100 on the nozzle contacts bracket 110 and thereby moves member 138 inwardly of switch 126. The downward movement of bracket 110 is accompanied by the downward movement of bracket .108 through the interconnection of these parts with links 114 and 116 and pins 118 and 124. .When members 130 and 138 have been moved downwardly far enough to open their respective switches the electrical circuit including these switches and solenoid 86 is opened and current stops flowing through that solenoid. Spring 184 then urges plunger 182 outwardly of solenoid 86 and moves block 78 by link 88. Air under pressure from compressor 74 then passes through air line 66 into the space in cylinder 34 below piston 38 forcing the piston upwardly.

As the piston moves upwardly it also carries nozzle 96 upwardly. As the nozzle moves upwardly, but before the tip of the nozzle is removed completely from within the soap beads contained within the carton, member 51 on arm 48 of elevator 46 moves away from trigger 170 whereupon spring 172 returns the trigger to its normal position shown in dotted lines thereby opening switch 7 169 and opening the circuit to solenoid 166. With the the position of rest beneath nozzle' 96 it will interrupt light beam 177.

The interruption of light beam 177 trips 'relay 180 and closes the electrical circuit including solenoid 86 and switches 126 and 128. Theclosing of this circuit energizes solenoid 86 whereby plunger 182 moves inwardly of the solenoid thereby causing link 88 to move block 78 on guide in such manner that the exit end of passage'84 in block 78 and the end 68 of line 64 are in registry, the end 70 of line'66 is open to the atmosphere, and the exit end of passage 82, is closed by block 11...

thin described air under pressurewill pass from cont:

opening of this circuit, spring 167 urges rod 164 outwardly of solenoid 166 whereupon needle 162 is seated and valve 160 is closed, the flow of material from cylinder 54 and through pipe 150 thus being stopped.

The use of switches 126 and 128 in a series circuit permits the circuit to be broken and nozzle. 96" to rise uninterruptedly on its return or upstroke. This is accomplished because although switch 126 is re-closed by the action of spring 132 soon after the upstroke begins, switch 128 re'rnains'open until the end of that stroke due to the linkage used. Thus, as nozzle 96 continues to move upwardly stop 1G0 moves away from bracket whereupon spring 13?. returns the bracket and member to their normal positions thereby closing switch 126. The upward movement of bracket 110 is not accompanied by the upward movement of bracket 108. Rather, pin '124 remains in its lowermostposition, indicated in dotted lines, as does bracket 108 and member 138, switch 128 remaining open.

However, as the nozzle 96 continues to move upwardly stop 100 thereon contacts bracket 108 and moves the same and member 138 upwardly, into the positions shown in solid lines, thereby closing switch 128.

After switch 126 has'been closed and before switch 128 is closed a predetermined quantity of soap beads will have been filled into the next carton through nozzle 14.

The mechanism. driving conveyor 16 then will start auto atis yfindca rr hg car n hus. filled .t om be th;

asap-19o:-

IIGZ'ZIQIJA .andtthefilled. and now-perfumed; carton from beneath nozzle 96;. Aftenthe filled and perfumed carton hasibeeny'conveyedfrom beneath nozzle 96, light beam 177-will= be received by photoelectric cell 178 whereby relay-18.0 :therein will open. By the time the filled and perfumed carton haspassedfrom beneath nozzle 96, the nozzle will have arrived at its'uppermost position whereupon switch 128willbe closed.

The parts will remain in the respective positions thus described until beam 177: again is interrupted. When conveyor 16 movesthe next filled carton into a position of rest-beneath nozzle 96 the carton will interrupt beam 177- closing the circuit including the solenoid 86 whereupon the novelsequence of steps in the operation will begin again; 7 r

The materials charged into cylinder-154 comprise, in general, solutions of pcrfurnes dissolved in a propellant which may beone or more liquefied gases. The perfumingmaterials may include any liquid perfume which is known in the art, Suitable examples include cinnamic alcohol, anisic aldehyde, hydroxycitronellal, eugenol, geraniol, coumarin, terpinol, oil of lavender, linalyl acetate, benzyl acetate, amyl salicylate, and oil of bergamot.

As propellants, any suitable liquefied, normally gaseous, organic material may be used. In general, said material should be substantially non-toxic, non-inflammable, lowboiling, and odorless. Specific examples of suitable propellants include liquefied. normally gaseous, low molecular weight halogenated hydrocarbon materials such as halogenated methane, ethane, propane, butane, and mixtures thereof.

Other halogenated hydrocarbon propellants which have been found to be particularly. suitable foruse in accordance with this invention include monochlorodifiuoromethane, monochlorodifiuoroethane, dichloromonofiuorocthane,, dichlopodifiuoromethane, dichlorotetrafiuoroethane, trichloromonofiuoromethane, and difluoroethane.

In some instances itmay be desirable touse a combination ot'ltwo or more of the liquefied, normally gaseous, materials as a propellant in order to achieve a suitable pressurewithinj cylinder 154 and impart the desired properties of stability, propellancy, and ease of delivery of the perfume composition to the detergent particles.

As indicated above the perfume composition comprises a solution of l perfume in propellant. In some instances,

using certain perfume materials, this solubility relationformulating the perfume composition to be introduced into cylinder 154 may be varied over a relatively wide range, Theamount of perfume employed depends primarily upontthcparticular perfumematerial used and the intensity of the odor it is desired toimpart to the detergent particles; The concentration of'perfume oil generally should amount to at least about 5%, usually about l to about 30%, and preferably about 15% to about 25% ofthe total weight of the composition in- 65 troduced into the cylinder.

'The amount of propellantused may be varied depending upon the. character of the detergent particles being zoates and,boratesnnay, be included to prevent corr'o.

sion of the various partsof the apparatus;

Cylinder 154 'may, be filled in any suitable manner. One convenient method comprises introducing the per-v fume into the cylinder, either alone, or in solution in alcohol or water or the like, and then sealing the cylinder, Thereafter, the propellant while under pressure may be admitted to the cylinder through valve 158 or other appropriate means, the cylinder being slightly chilled during this operation if desired. The chilling of the cylinder permits it to be charged under conditions which provide a greater available'propelling pressure when the cylinder regains atmospheric temperature.

Another satisfactory filling method comprises prechilling the mixture of all the ingredients to a temperature below the boiling point of the propellant and then charging said ingredients into the cylinder which is sealed thereafter.

The amount of the perfume composition introduced 20.;interiorly into a given mass of particulate material depends upon the particular perfume and propellant used, the specific detergent material being perfumed, and the amount of such detergent material contained within the package or carton.

above the apparatus preferably is arranged in such manner that about one-half cubic centimeter of the perfume composition is ejected into each carton containing about ounces of the beads. Preferably about one-quarter I -cubic centimeter of the perfume composition is ejected into the. carton during the downward movement of the nozzle 96 and, about one-quarter cubic centimeter is I uniform distribution of aromatic oils, fats, and like liquids into particulate powdered products of various kinds.

Furthermore, While the present invention has beendisclosed and described with reference to particular erobodiments thereof, it will be understood, of course, that many modifications and changes and substitutions may be made therein without departing from the true scope of the invention as defined in the appended claims. 7 Having thus described the invention, what is claimed is: 1. Apparatus for automatically perfuming with a predetermined amount of perfume, a given quantity of detergent particles contained within a package, comprising a gas-tight container for a liquid mixture of perfume and liquefied normally gaseous propellant under pressure, a

longitudinally extending, vertical nozzle in flexible com-- munication with the gas tight container'at one end and having an outlet orifice at its other end, a solenoid valve intermediate the orifice and container, an air cylinder, a pistonadapted to reciprocate within the cylinder, a source of compressed air communicating with the air cylinder near the ends thereof, a sliding-block valve for directing 0 compressed air alternately to the ends of the cylinder and for exhausting air from';.the opposite end, thereby causing the piston to reciprocate within the cylinder, at source of electric power, an electric switch in series with the source of electric power and, the solenoid valve, an arm operatively. connecting the :piston and nozzle and adapted to move the nozzle orifice into the package, substantially through the height of detergent particles and back out'of the package as the piston reciprocates said arm comprising an actuating member, adapted to close the circuit and therebyv to open the solenoid valve, allowing the passage of perfume mixture through the nozzle and into the pack; age of detergent when the nozzle orifice is descending below the surface of the detergent particles, theactuating -member-also beingadaptedtoopen the circuit, thereby" When perfuming soap beads of the character described 7 closing the solenoid valve, when the nozzle orifice is rising'and below the surface of the detergent particles, the dispensing of perfume being continuous substantially throughout the height of detergent in the package, a stop actuator atfixed to the nozzle, a solenoid for moving the sliding-block valve and thereby causing reciprocation of the piston, a photoelectirc switch in the solenoid circuit which closes only when a package interrupts its light beam, said interruption occurring only when said package is in position to be perfumed, a pair of switches actuated by the stop actuator, which switches are an upper twoposition unbiased switch having an actuating member extending downwardly which switch is closed when the member is moved upwardly, a lower biased normally closed switch having an actuating member extending upwardly which switch is opened when the actuating member is moved downwardly, a linking member connecting the actuating member of the upper switch with the actuating member of the lower switch, the actuating members of said switches being so made that the lower switch, when in the open position, will open the upper switch by means of the linking member and when in the closed position, will allow the upper switch to remain open unless the upper switch is acted upon by an outside force, namely the stop actuator affixed to the nozzle, the actuating members of the upper and lower switches being movable directly upwardly and downwardly by the movement of the stop actuator, so that when there is a package of detergent in perfuming position the nozzle will descend into the package, discharge perfume in propellant and withdraw, and an automatic conveyor which intermittently moves and rests and which is adapted to move a package of detergent material into position underneath the upraised filling nozzle, maintain it there for the time required for perfuming the package and then remove saidpackage from the perfuming area and replace it with another.

2. Apparatus for automatically perfuming with a predetermined amount of perfume, a given quantity of detergent particles in a package, comprising a gas-tight container for a liquid mixture of perfume and liquefied normally gaseous propellant under pressure, a longitudinally extending vertical nozzle in communication with the gastight container and having an outlet orifice, a valve intermediate the orifice and container, an air tube, a piston adapted to reciprocate within the tube, a source of compressed air communicating with the air tube near the ends thereof, a valve for directing the compressed air alternately to the ends of the tube and for venting the opposite end, thereby causing the piston to reciprocate within the tube, means operatively connecting piston and nozzle to transmit to the nozzle a reciprocating motion and move the nozzle orifice into the package substantially through the height of detergent particles and back out of the package, an actuating member operatively connected with reciprocating nozzle, means, actuated by the said member, for opening the valve intermediate orifice and container when the nozzle is descending and below the surface of the detergent particles and for closing said valve when the nozzle is ascending and below said surface, thereby allowing continuous perfuming substantially through the height of detergent in the package, actuating means operatively connected with the nozzle and adapted to automatically operate the valve for directing compressed air in such a manner that air will be passed into the end of the tube which will cause the nozzle to move downwardly when the nozzle is at a pre-set upper limit above the top of the package and air will be passed into the other end to direct the nozzle upwardly when said nozzle is at a pre-set lower limit near the bottom of the package, means for preventing the descent of the nozzle when the space under the nozzle, the perfuming position, is unoccupied'by a package of detergent and an automatic conveyor which intermittently moves and rests and which is adapted to move a package of detergent material into quired to perfume the package, remove said package from the perfuming position and replace it with another.

3. Apparatus for automatically distributing a prede termined amount of a liquid in a given packaged mass of particulate material comprising a gas-tight container for a liquid mixture of the liquid to be distributed, and a liquefied normally gaseous propellant under pressure, a nozzle in communication with the gas-tight container and having an outlet orifice, a valve intermediate orifice and container, means for lowering and elevating the nozzle relative to the package so that the orifice alternately descends into the package to near the bottom thereof and ascends above the package, means synchronized with the nozzle to open the valve when the orifice is below the surface of the mass of particulate material and to close the valve when the orifice is above said surface, thereby releasing the liquid mixture through the orifice substantially throughout the height of the particulate mass and only when said orifice is beneath the particulate material, and an automatic conveying device adapted to move a package of particulate material into position under the nozzle while the nozzle is raised, maintain it therefor the time required to add the liquid mixture, remove the package and replace it with another.

4. A process for distributing a liquid in a mass of particulate material which comprises making a solution of the liquid in a liquefied normally gaseous propellant, introducing a quantity of said solution into a restricted passageway having an outlet of cross-sectional area substantially less than the cross-sectional area of the mass of particulate material and conducting the liquid, with the aid of the propellant, through the passageway out the outlet and into the interior of the mass of particulate material when the outlet is within said interior.

5. A process for distributing a liquid in a given mass of substantially quiescent particulate material which comprises making a solution of the liquid in a liquefied normally gaseous propellant, introducing a predetermined quantity of said solution into a restricted passageway having an outlet of cross-sectional area substantially less than the cross-sectional area of the mass of particulate material and conducting the liquid, with the aid of the propellant, through the passageway out the outlet and into the interior of the mass of particulate material, the solution of liquid in propellant being at a pressure above atmospheric while in the restricted passageway, due in substantial part to the vapor pressure of the propellant and the discharge of the solution into the mass of particulate material being as a spray caused by release of pressure as the solution leaves the restricted passageway.

6. A process for perfuming a previously packaged given mass of detergent material which comprises male ing a solution of perfume in a liquefied normally gaseous propellant, introducing a predetermined quantity of said solution into'a restricted passageway having an outlet of cross-sectional area substantially less than the crosssectional area of the packaged mass and conducting the perfume, with the aid of the propellant, through the passageway out the outlet and into the interior of the mass of particulate detergent when said outlet is within said interior.

7. A process for perfuming a previously packaged given mass of particulate detergent material which comprises making a solution of perfume in a suitable liquefied normally gaseous propellant, introducing a predetermined quantity of said solution into a restricted passageway having an outlet of cross-sectional area substantially less than the cross-section area of the packaged mass and conducting the perfume, with the aid of the propellant, through the passageway out the outlet and into the interior of the mass of particulate detergent while moving the passageway and outlet through the mass of particulate material, the perfume solution being at a pressure above atmospheric while in the restricted P sa way,, e n ub. a t a par to apor, p e suy e efethe, pl epellant, and thediseh arge 0f, the sol-utiqn te .6, mas o par w a detergent n a $923! caused by release-of pressure as the sblution leaves the restricted passageway.

References Cited in they file of this patent UNITED STATES PATENTS 361,930 Collins Apr. 26, 1887 940,366 Sehlahgen Nov. 16, 1909 1,346,948 Freedmari July 20, 1920 1,34,6 53 Taliaferro Jan. 4, 1921 12 Heath et al Feb. 14, 1922 Gpttseha lk Apr. 7,1925 Rotheim Jan. 3; 193 3 Iddings Feb. 9, 1937 V Bae ehle etl Sept. 17, 1944 Harms Feb. 26, 1952 Lutz Nov. 11, 1952 McB ean June 9, 1953 Martin Aug. 11, 1953 'Plusquellic Apr. 6, 1954 Nielsson Ian. 3, 1956 

